Chapas laminadas a quente com 6 mm de espessura dos aços AISI 304L e 316L apresentaram na condição inicial uma microestrutura composta por grãos recristalizados equiaxiais de austenita e ilhas de ferrita δ, em maior quantidade no centro da chapa. A austenita apresentou textura cristalográfica fraca, com um gradiente de textura ao longo da espessura. Os tratamentos térmicos de solubilização causaram a eliminação da ferrita, mas não causaram modificação substancial na textura. Os fenômenos de encruamento, recuperação e recristalização foram então estudados após solubilização, seguida de deformação por laminação em diferentes temperaturas e posterior recozimento das amostras deformadas. O endurecimento por deformação e a porcentagem de martensita α’ formada mostraram forte dependência com a composição química da austenita e com a temperatura de deformação. A textura de deformação encontrada nos aços inoxidáveis austeníticos 304L e 316L é característica dos materiais CFC com baixa e média energia de empilhamento laminados a frio. A temperatura de reversão da martensita α’ foi próxima de 550°C, praticamente não depende da quantidade presente e é praticamente idêntica nos dois aços. O aço 316L apresentou maior resistência à recristalização, pois tem maior EDE e apresenta menor endurecimento por deformação em relação ao 304L. A temperatura de recristalização situouse aproximadamente 150°C acima da temperatura de reversão da martensita α’. A temperatura de laminação não influenciou significativamente a temperatura de recristalização. A textura de recristalização nos dois aços continuou sendo semelhante à textura de deformação. As propriedades mecânicas de tração dos dois aços mostraram-se muito sensíveis à temperatura do ensaio. Tratamentos mecânicos e térmicos adequados produziram combinações interessantes de propriedades mecânicas nos dois aços, tais como limite de escoamento por volta de 1000 MPa com alongamento da ordem de 10%. Os resultados do presente trabalho sugerem que para se obter nos aços inoxidáveis austeníticos combinações atrativas de alta resistência mecânica com ductilidade razoável, por meio de tratamentos mecanotérmicos ou termomecânicos, duas diretrizes devem ser observadas: i) durante a deformação grandes quantidades de martensita devem ser produzidas e as principais variáveis neste aspecto são a EDE do aço e a quantidade e a temperatura de deformação; ii) durante o recozimento do material encruado deve ocorrer reversão da martensita, mas a recristalização completa deve ser evitada, por meio do controle rigoroso da temperatura e do tempo de recozimento, obtendo-se uma microestrutura muito fina de grãos e sub-grãos. A possibilidade de tratamentos sucessivos de deformação/recozimento é promissora e deve ser explorada em trabalhos futuros. A caracterização microestrutural foi realizada com auxílio de várias técnicas complementares de análise microestrutural, tais como microscopia óptica, microscopia eletrônica de varredura (MEV), microscopia eletrônica de transmissão (MET), medidas magnéticas, difração de raios X (análise de fases e determinação de textura) e microdureza Vickers. A caracterização mecânica envolveu a realização de ensaio de tração em várias temperaturas, com a determinação de limite de escoamento, limite de resistência, alongamento total e coeficiente de encruamento n. / Hot rolled AISI 304L and 316L austenitic stainless steel sheets, 6mm thick, presented recrystallized equiaxial grains with austenite and islands of delta ferrite, in larger quantities mainly in the center of both steel sheets. The austenite had a weak texture, with a gradient through the thickness. The solution annealing eliminated delta ferrite, however it did not change the texture. Phenomena such as work hardening and strain induced α’ martensite formation showed strong dependency on the chemistry composition and rolling temperature. The rolling texture observed in AISI 304L and 316L austenitic stainless steels is characteristic of FCC materials with low and medium stacking fault energy (SFE), after cold rolling. The α’ reversion temperature was around 550°C for both steels and was independent of the volume fraction of α’ martensite. The AISI 316L showed a strong recrystallization resistance as it has higher SFE and smaller work hardening than the AISI 304L. The recrystallization start temperature is approximately 150°C higher than the α’ reversion temperature. The rolling temperature did not influence the recrystallization temperature. Recrystallization texture for both steels remained similar to the rolling texture. Proper thermal and mechanical treatments provided interesting combinations of mechanical properties for both steels, such as yield strength around 1000 MPa with 10% elongation. These results suggest that the obtained austenitic stainless steels provide attractive combinations not only with high mechanical resistance but also with reasonable toughness and ductility. Through thermo-mechanical treatments, two point must be stressed: i) during the deformation great quantities of α’ martensite are being produced due to the SFE of the steel and the degree and the temperature of deformation; ii) during the annealing treatment of the work hardened material the α’martensite reverts to austenite, but complete recrystallization must be avoided, thus strict control of temperature and annealing time must be ensured to obtain a refined microstructure (of grains and subgrains). The possibilities of employing successive deformation / annealing treatments is promising and should be explored in future research. Several microstructural characterization techniques have been employed: optical microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), magnetic measurements, X-ray diffraction to analyze phases and textures, and Vickers microhardness tests. Mechanical characterization involved tensile testing at different temperatures, with determination of yield strength, tensile strength, total elongation and strain hardening coefficient n.

Os aços inoxidáveis austeníticos são materiais atrativos para serem utilizados em vários setores industriais que operam sob meios corrosivos, como por exemplo: indústria química, alcooleira, petroquímica, de papel e celulose, na prospecção de petróleo e nas indústrias têxtil e farmacêutica. Contudo, apresentam propriedades tribológicas pobres. No sentido de melhorar essas propriedades, como aumentar a dureza superficial, a resistência ao desgaste e a resistência à fadiga, vários métodos de tratamentos superficiais vêm sendo utilizados. Dentre eles, o mais eficiente é a nitretação por plasma. Este processo é realizado em uma câmara de vácuo sob uma mistura gasosa de hidrogênio e nitrogênio. É aplicada uma diferença de potencial entre o cátodo (porta amostras) e o ânodo (paredes da câmara), acelerando os íons contra a superfície da peça, aquecendo-a e arrancando elétrons de sua superfície. Os íons reagem com espécies da superfície do plasma formando compostos instáveis do tipo FeN que se recombinam para formarem nitretos estáveis. O sucesso deste tratamento se deve à baixa temperatura de operação, ao menor tempo efetivo de tratamento e ao controle da uniformidade da espessura da camada. A camada de nitretos formada durante o tratamento possui uma influência positiva na vida em fadiga de um componente, graças a dois motivos principais. O primeiro é o atraso na nucleação da trinca devido ao aumento da resistência mecânica superficial. O segundo motivo está relacionado com a introdução de tensões residuais compressivas durante o processo de endurecimento da superfície, que retarda a iniciação da trinca e diminui o fator de intensidade de tensão. Os corpos de prova foram nitretados a 400ºC durante 6 horas, com uma pressão de 4,5 mbar e utilizando uma mistura gasosa de 80% vol.H2 e 20%vol.N2. Ocorreu um aumento da resistência mecânica próxima á superfície, devido à camada de nitretos, o que ficou evidente com o sensível aumento no valor do limite de fadiga do material nitretado em relação ao não nitretado. O limite de fadiga do aço AISI 316 não tratado foi de 400MPa e do nitretado foi de 510MPa, enquanto que, para o aço AISI 304, o limite de fadiga do material não tratado foi de 380MPa e o limite para material submetido ao tratamento de nitretação foi de 560MPa. / The austenitic stainless steels are attractive materials to many industrial sectors which work on corrosive environments, as chemical industry alcohol, petrochemical, cellulose industries, in the petroleum prospection and pharmaceutical and textiles industries. However, they present poor tribological properties. In order to improve these properties, like increasing superficial hardness, wear and fatigue resistance superficial heat treatment methods have being used. The most efficient is the plasma nitriding process which occurs in a vacuum container under hydrogen and nitrogen gas mixture. A potential difference is applied between the cathode (samples receptor) and the anode (container walls), accelerating the ions against the piece, heating it and removing electron from the surface of material. These atoms react with the surface plasma species, producing unstable compounds like FeN, which recombine producing stable nitrides. The success of this treatment is due to the low temperature operation, the short effective time of treatment and to the uniformity control of the layer’s thickness. The nitrides layer produced during the treatment have a positive influence in the fatigue life of a component, thanks to two main reasons. The first is the retardation in crack nucleation due to increasing of superficial mechanical strength. The second reason is due to introduction of compressive residual stress during the surface hardening process, which retards de crack initiation process. The specimens were nitriding at 400°C during 6 hours, at a 4,5mbar pressure and using a gas mixture of 80% vol. H2 and 20% vol. N2. The surface mechanical strength increased, due to the nitrides layer, which was evident with the sensitive increase in the fatigue limit of the nitriding specimens, comparing to the untreated ones. The fatigue limit of the AlSl 316 steel in untreated condition was 400 MPa and in nitriding condition was 510 MPa, whereas AlSl 304 steel, the fatigue limit of the untreated condition was 480 MPa and the fatigue limit for the nitrided condition was 560 MPa.

A busca por alternativas para aumentar a resistência à oxidação ao ar a altas temperaturas de metais e ligas aumenta a cada dia, devido à necessidade de otimização da vida útil dos equipamentos que operam nestas condições. Novos materiais projetados para trabalhar nestas condições possibilitam reduzir custos de manutenção, aumentando a produtividade dos equipamentos, devido à redução do tempo de paradas programadas. O uso de aços inoxidáveis microligados a elementos terras raras é uma das alternativas adotadas, por exemplo, para tubulações para a indústria de petróleo e gás. Este trabalho estuda a resistência à oxidação ao ar a altas temperaturas de juntas soldadas de um aço inoxidável austenítico microligado ao cério. As juntas soldadas foram confeccionadas através do processo de soldagem MIG/MAG, depositando-se cordões de solda em chapas de aço inoxidável austenítico AISI 304L, variando-se a composição dos gases de proteção e mantendo-se os outros parâmetros de soldagem. Amostras dos diferentes metais depositados foram preparadas através de corte com disco diamantado e submetidas a ensaios de oxidação a altas temperaturas ao ar em balança termogravimétrica. Os corpos de prova oxidados foram estudados usandose microscópio óptico, microscópio eletrônico de varredura com EDS e difração de raios X. Observaram-se cinéticas de oxidação parabólicas em todas as temperaturas estudadas: 800, 900, 1000 e 1100 °C. Os Kps encontrados neste trabalho reforçam a tese de que ocorra a formação de películas protetoras de Cr2O3 e SiO2, o que reforça a hipótese que as mesmas tenham sido efetivamente formadas após os estágios iniciais de oxidação. Em todos os corpos de prova oxidados ao ar nas diferentes temperaturas, observou-se a formação de uma película não protetora de óxidos de ferro (Fe2O3, Fe3O4 e FeO) e posterior formação de uma camada protetora mais espessa de crômia (Cr2O3). Mais internamente observou-se a formação de SiO2. / The search for alternatives to increase the high temperatures oxidation resistance in air of metals and alloys increases every day due to the need to optimization of the life expectancy of equipment operating in these conditions. New materials designed to work in these conditions make it possible to reduce maintenance costs, increasing productivity of equipment due to reduced shutdowns. The use of austenitic stainless steel microalloyed with rare earth elements is adopted an alternative, for example, to tubes and pipes for the oil and gas industry. This work aims to study the high temperature oxidation resistance in air of welded joints of an austenitic stainless steel microalloyed with cerium. The welded joints were welded using MIG / MAG welding process, depositing weld beads on a sheet of austenitic stainless steel AISI 304L by varying the composition of the shielding gases. Samples of the different welded joints were prepared by cutting with a diamond disk and were subjected to high temperatures oxidation testing in thermogravimetric balance. The oxidized specimens were studied using optic microscopy, scanning electron microscope with EDS and Xray diffraction. Parabolic oxidation kinetics were observed at all temperatures studied: 800, 900, 1000 and 1100 °C. The Kps found in this work reinforce the thesis that the formation of protective films of Cr2O3 and SiO2 occurs, reinforcing the hypothesis that they have been effectively formed after the initial stages of oxidation. In all specimens oxidized at different temperatures, a formation of a non-protective layer of iron oxides (Fe2O3, Fe3O4 and FeO) and subsequent formation of a thicker protective layer of chromite (Cr2O3) was observed. More internally, SiO2 formation was observed.

A combination of fractography, microstructural analysis and finite element modelling was used to investigate several topics relating to the fatigue of nuclear grades of austenitic stainless steel operating in both air and simulated PWR water environments. The work is broadly separated into four main categories. The first two involved analysing specimens from standard fatigue endurance tests using a wide range of microscopic techniques. The relevance and uses of a modern laser scanning confocal microscope are presented and the benefits of using such a technique are discussed. Methods for the automation of both striation counting procedures and hysteresis data analysis are described and the results are demonstrated. Finite element analyses were performed in order to develop the understanding of fatigue crack growth within standard cylindrical endurance specimens. A variety of different crack tip parameters were used in order to develop expressions for crack growth rates in terms of the strain intensity factor and the J-integral. The derived expressions were compared to the results of striation spacing measurements from multiple endurance specimens that were tested in both air and water environments. The expressions were used to perform back-fitting calculations on standard endurance curves in order to produce alternative curves representing the number of loading cycles to cause the initiation of short cracks with depths in the range of 0.25-0.5 mm. The effects of hold-times on the fatigue life of stainless steel endurance specimens were explored as part of the international AdFaM research programme. Results from the programme partners are presented which demonstrate the beneficial effects of static hold-times on extending the fatigue lifetime of specimens. A range of microstructural analyses were performed on test specimens and results are presented. No significant effects of hold-times on microstructure, crack growth rates or material hardness were found. Analysis of hysteresis data demonstrated an increase in the cyclic hardening and a decrease in the plastic strain range after a hold. From an analysis of the fatigue test results, it was concluded that hold-times affect the earliest stages of fatigue (nucleation and initiation), most likely due to the effects of strain ageing. Several possible explanations for the observed phenomenon of specimen shrinkage during static holds are presented and discussed, however no conclusive explanation was identified. Further work is identified that could lead to future improvements in the understanding of all areas of investigation that have been reported. Overall, the work reported here has helped to develop the understanding of fatigue behaviour and mechanisms in the materials of interest. This was done through investigations using a synergistic combination of microscopy and numerical modelling techniques.

Orientador: Carlos Roberto Grandini / Banca: Eduardo Carlos Bianchi / Banca: Cristina de Carvalho Ares Elisei / O Programa de Pós-Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi da Unesp / Resumo: Os elementos intersticiais exercem uma influência significativa nas propriedades mecânicas dos materiais e seu comportamento pode ser investigado por meio de técnicas de Espectroscopia Mecânica em baixa frequência (Pêndulo de Torção). Nestas medidas, são obtidos espectros de atrito interno, que estão associados à reorientação de elementos intersticiais presentes no material ao se aplicar uma tensão mecânica (fenômeno induzido). As amostras utilizadas neste trabalho são de aço inoxidável 316L obtido comercialmente. O material foi preparado em quatro condições: como recebido, tratado termicamente e duas dopagens com pressões diferentes de nitrogênio. Para caracterizar o material foram realizadas medidas de densidade, difração de raios X, microscopia eletrônica de varredura, espectroscopia de energia dispersiva e espectroscopia mecânica. As medidas de difração de raios X e microscopia eletrônica de varredura revelam que as amostras possuem uma estrutura CFC, típica de aços austeníticos. Os espectros de atrito interno das amostras revelam algumas estruturas de relaxação em todas as condições de tratamento, medidas em três diferentes frequências. Essas estruturas foram decompostas em seus processos de relaxação constituintes, associados à reorientação induzida por tensão de elementos intersticiais, como o carbono e nitrogênio, em torno de átomos que compõem o material. A comparação dos espectros de relaxação obtidos em cada condição mostra uma perda na intensidade das estruturas após realizar sucessivas medidas. Os resultados levam a concluir que este fenômeno está relacionado com a perda de elementos intersticiais pelas amostras após o aquecimento em vácuo. / Abstract: The intersticial elements exercise a significant influence in the mechanical properties of the materials and its behavior can be investigated by techniques of mechanical spectroscopy in low frequency (Torsion Pendulum). In these measurements, are obtained internal friction spectra, which are associated to the reorientation of interstitial elements present in the material if applied a mechanical stress (induced phenomenon). The samples used in this study are commercially 316L stainless steel. The material was prepared in four conditions: as received, heat treated and doped with two different pressures of nitrogen. To characterize the material, it was made measurements of density, x-ray diffraction, scanning electronic micrsocopy, electron dispersion spectroscopy and mechanical spectroscopy. The measurements of x-ray diffraction and scanning electronic microscopy reveal that the samples have a CFC structure, typical of austenitic steels. The internal friction spectra, measured in three different frequencies, reveal several relaxation structures in all of the conditions. Those structures were decomposed in their constituent relaxation processes, associates to the stress-induced ordering of interstitial elements, as carbon and nitrogen, around atoms that compose the material. The comparason of the relaxation spectra obtained in each condition shows a loss in the intensity of the relaxation structures after successive measurements. The results take to conclude that this phenomenon is related with the loss of interstitial elements of the samples after the heating in vacuum. / Mestre

Os aÃos inoxidÃveis austenÃticos (AIAs) sÃo largamente aplicados nas indÃstrias de alimentos, transportes nuclear, petroquÃmica devido à adequada combinaÃÃo de resistÃncia mecÃnica, conformabilidade e resistÃncia à corrosÃo. Dentre estes tipos de aÃo, destaca-se o AISI 301 por sua resistÃncia mecÃnica superior. Entretanto, este tipo de aÃo apresenta um dos piores desempenhos em termos de corrosÃo. Toda a resistÃncia à corrosÃo dos AIAs se baseia em sua camada de filme passivo contendo Cr203 que pode facilmente ser destruÃda em ambientes contendo cloreto. Neste trabalho, estabeleceu-se a meta de estudar os aÃos AISI 301 LN e 316L em respeito Ãs mudanÃas na microestrutura por imposiÃÃo de deformaÃÃo e seu efeito na corrosÃo por pites, visto que o AISI 301LN foi escolhido como material base dos vagÃes que servirÃo o sistema de transporte metropolitano de Fortaleza. Empregou-se difraÃÃo de raios âX, metalografia quantitativa, microscopias Ãtica, eletrÃnica de varredura e de forÃa atÃmica para caracterizar a microestrutura, textura cristalogrÃfica, caracterizaÃÃo magnÃtica, microdureza e ensaio de imersÃo em FeCl3 6H2O para caracterizar o comportamento dos dois aÃos em corrosÃo por pites. A deformaÃÃo provocou a formaÃÃo de martensita â no aÃo 301LN e encruamento da austenita. Isto provocou o mais baixo desempenho em corrosÃo por pites. A textura cristalogrÃfica forneceu indÃcios para inferir que a transformaÃÃo austenita-ferrita se deu obedecendo a relaÃÃo de KURDJUMOV-SACHS.

Bridges and other coastal structures in Georgia and throughout the Southeast are deteriorating prematurely due to corrosion. Numerous corrosion initiated failures have occurred in precast prestressed concrete (PSC) piles and reinforced concrete (RC) pile caps, leading to the costly repair and replacement of either the entire bridge or the affected members. With the Federal Highway Administration's goal of a 100-year bridge service life and recent legislative action such as the Bridge Life Extension Act, new emphasis has been placed on the development and implementation of new corrosion mitigation techniques. This thesis involves the mechanical testing, and proposed future test program of high-strength stainless steel (HSSS) prestressing strand to be used in prestressed marine bridge piles. The metallurgy for two types of HSSS strand was selected from a previous study of the corrosion resistance, mechanical properties, and feasibility of 6 candidate HSSS drawn wire samples. Duplex stainless steel (DSS) grades 2205 and 2304 were selected for production of 7-wire 1/2" diameter prestressing strand. DSS wire rod was drawn, stranded, and heat-treated using the same production methods and equipment as used for standard of practice, high carbon prestressing strand. The production process was documented to analyze the problems facing this production method and suggest improvement and optimization. After production, the strands were subjected to a series of mechanical tests. Tension testing was performed to provide a stress-strain curve for the strands and related mechanical properties. Wire samples were also taken at varying points in the drawing process to give more information about the work hardening of the stainless steels. Stress relaxation testing was performed on both strand and wire samples to assess the overall losses and to provide comparisons between strand and wire test results as well as drawn wires before and after heat-treatment. An experimental program for future study was designed to assess the HSSS prestressing strand behavior in precast piles. This testing involves assessment of pile driving performance, pile flexural and shear behavior, strand transfer and development length, long-term prestressing force losses, and material durability.

No description available.

Ferritic stainless steels are the most commonly used materials for solid oxide fuel cell interconnect application. Although these alloys may meet the criteria for interconnect application for short periods of service, their application is limited for long-term use (i.e., 40,000 h) due to poor oxidation behaviour that results in a rapid increase in contact resistance. In addition, volatile Cr species migrating from the chromia scale can poison the cathode resulting in a considerable drop in performance of the cell. Coatings and surface modifications have been developed in order to mitigate the abovementioned problems. In this study, composite electrodeposition of reactive element containing particles in a metal matrix was considered as a solution to the interconnect problems. Nickel and Co were used as the metal matrix and LaCrO3 particles as the reactive element containing particles. The role of the particles was to improve the oxidation resistance and oxide scale adhesion, while the role of Ni or Co was to provide a matrix for embedding of the particles. Also, oxidation of the Ni or Co matrix led to the formation of conductive oxides. Moreover, as another part of this study, the effect of substrate composition on performance of steel interconnects was investigated. Numerous experimental techniques were used to study and characterise the oxidation behaviour of the composite coatings, as well as the metal-oxide scale interface properties. Scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDX), as well as surface analysis techniques including Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectroscopy (SIMS), were used for the purpose of characterization. The substrate used for coating was AISI-SAE 430 stainless steel that is considered as a typical, formerly used interconnect material. Also, for the purpose of the metal-oxide scale interfacial study, ZMG232 stainless steel that is a specially designed interconnect alloy was used. It is shown that the composite coatings greatly reduce the contact resistance and effectively inhibit Cr outward migration. In addition, it was determined that the presence of impurities in the steel, especially Si, and the absence of reactive elements drastically contribute to interconnect degradation. / Materials Science and Engineering

Bulk nanocrystalline 304L and 316L austenitic stainless steels (SS) were produced by equal channel angular pressing(ECAP) at elevated temperature. The average grain size achieved in 316L and 304 L SS is ~ 100 nm, and grain refinement occurs more rapid in 316 L SS than that in 304L. Also the structures are shown to retain a predominant austenite phase. Hardness increases by a factor of about 2.5 in both steels due largely to grain refinement and an introduction of a high density of dislocations. Tensile strength of nanocrystalline steels exceeds 1 GPa with good ductility in both systems. Mechanical properties of ECAPed 316L are also shown to have less dependence on strain rate than ECAPed 304L. ECAPed steels were shown to exhibit thermal stability up to 600oC as indicated by retention of high hardness in annealed specimens. Furthermore, there is an increased tolerance to radiation-induced hardening in the nanocrystalline equiaxed materials subjected to 100 keV He ions at an average dose of 3-4 displacement-per-atom level at room temperature. The large volume fraction of high angle grain boundaries may be vital for enhanced radiation tolerance. These nanocrystalline SSs show promise for further research in radiation resistant structural materials for next-generation nuclear reactor systems.